电感耦合等离子体原子发射光谱法测定镧铁合金、铈铁合金和镧铈铁合金中主量稀土  

Determination of major rare earth in lanthanum ferroalloy,cerium ferroalloy and lanthanum-cerium ferroalloy by inductively coupled plasma atomic emission spectrometry

作　　者：于亚辉[1,2] 王素梅[1,2] 张秀艳[1,2] 刘丹娜 包香春[1,2] YU Yahui;WANG Sumei;ZHANG Xiuyan;LIU Danna;BAO Xiangchun(State Key Laboratory of Rare Earth Resources Research and Comprehensive Utilization,Baotou Research Institute of Rare Earths,Baotou 014030,China;Ruike National Engineering Research Center of Rare Earth Metallurgy and Functional Materials,Baotou 014030,China)

机构地区：[1]包头稀土研究院白云鄂博稀土资源研究与综合利用国家重点实验室,内蒙古包头014030 [2]瑞科稀土冶金及功能材料国家工程研究中心,内蒙古包头014030

出　　处：《冶金分析》2023年第3期40-44,共5页Metallurgical Analysis

摘　　要：镧铁合金、铈铁合金和镧铈铁合金主要用作钕铁硼永磁材料或钢铁材料的稀土添加剂,而快速准确测定镧铁合金、铈铁合金和镧铈铁合金中主量稀土含量对产品的质量控制具有重要意义。采用盐酸-过氧化氢溶解样品,选择La 492.098 nm、Ce 447.124 nm为分析谱线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定镧铁合金、铈铁合金和镧铈铁合金中主量稀土的分析方法。讨论了基体浓度、共存元素干扰等对测定的影响。结果表明,当铁质量浓度不大于0.2 mg/mL和镧(铈)质量浓度不大于20μg/mL时,基体效应可以忽略。样品中共存稀土元素和钙、镁、铝、锰、镍、硅、硫、磷等非稀土元素对稀土测定的影响可以忽略。镧、铈质量浓度在1.00~20.00μg/mL范围内与其对应的发射强度呈线性关系,校准曲线线性相关系数均为0.9999。按照实验方法测定镧铁合金样品中镧,铈铁合金样品中铈,镧铈铁合金样品中镧、铈,结果的相对标准偏差为(RSD,n=11)均小于3%。按照实验方法测定镧铁合金、铈铁合金和镧铈铁合金内控样品的主量稀土含量,结果与草酸盐重量法测定结果一致。Lanthanum ferroalloy(LaFe),cerium ferroalloy(CeFe)and lanthanum-cerium ferroalloy(LaCeFe)are mainly used as the rare earth additive for neodymium-iron-boron(NdFeB)permanent magnet materials or steel materials,and it is of great significance to determine major rare earth rapidly and accurately in LaFe,CeFe and LaCeFe for the product quality control.After the sample was dissolved with hydrochloric acid and hydrogen peroxide,a method for determination of major rare earth in LaFe,CeFe and LaCeFe was established by inductively coupled plasma atomic emission spectrometry(ICP-AES)with La 492.098 nm and Ce 447.124 nm as the analytical lines.The effect of matrix concentration and coexisting elements on the determination was discussed.The results showed that the matrix effect could be neglected when the mass concentrations of iron and lanthanum(cerium)were not more than 0.2 mg/mL and 20μg/mL,respectively.The influence of coexisting rare earth elements and non-rare earth elements(including calcium,magnesium,aluminum,manganese,nickel,silicon,sulfur and phosphorus)in the sample on the determination of major rare earth could be ignored.The mass concentration of lanthanum and cerium in range of 1.00-20.00μg/mL were linear with their corresponding emission intensity,and the linear correlation coefficients for calibration curves were all 0.9999.The proposed method was applied for determination of lanthanum in LaFe,cerium in CeFe as well as lanthanum and cerium in LaCeFe,and the relative standard deviations(RSD,n=11)were all less than 3%.The contents of major rare earth in internal control samples of LaFe,CeFe and LaCeFe were determined according to the proposed method.The results were consistent with those obtained by oxalate gravimetric method.

关 键 词：电感耦合等离子体原子发射光谱法(ICP-AES) 镧铁合金 铈铁合金 镧铈铁合金 镧 铈 

分 类 号：O657.31[理学—分析化学] TG115.33[理学—化学] TF845[金属学及工艺—物理冶金]